Distillation process.



S. NEAL. DISTILLATION PROCESS.

APPLICATION FILED APR. 17, 1909.

Patented Aug. 20, 1912.

' rior product will be produced. The process STEPHENS NEAL, OF OOBDELE, GEORGIA,

COMPANY, OF

ASSIGNOR T0 THE NEAL NAVAL STORES CORDELE, GEORGIA, A CORPORATION OF GEORGIA. v

' DISTILLATION PROCESS.

To all whom t may concern.'

Be it known that I, STEPHENS NEAL, a citizen of the United States, residing `at Cordele, in the county of Crisp and State of Georgia, have invented certain new and. useful Improvements in Distillation Processes; and `1 do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

My invention relates to improvements in distillation processes and is especially intended for use in the production of tui-pentine and rosin.

It is well understood in turpentine distillation that to obtain a good quality of rosin it is necessary that the crude gum should not become charred or carbonized during the distillation process. It is further wellknown that while distilling crude, raw material the uncombined water and lighter oils first come over very readily when a temperature of about 2120 F. is reached. When the temperature, however, is raised less volatile oils come olf until a temperature of say about 2650 F. is reached when I add water and the distillation continued. It is further well known that if the temperature is allowed to rise too high, the rosin will become charred and an infeof distilling turpentine, however, for com mercial reasons, is carriedA on with very cheap labor, and these operatives generally determine when to stop the distillation process by listening to the worm to ascertain whether or not ebullition in the still has ceased. This method, however, as will be apparent, is very crude and the result is but very often an inferior quality of rosin. As a matter of fact, even were the workmen better skilled, it would be impossible for them to tell from the sounds inside the still whether or not a charring had taken place or was about to take place in the rosin to be produced. All that can be determined by the present custom of listening to the worm, is whether or not the prod; uct is slowly boiling or is vigorously boiling.

y Specification of Letters Patent.

Application filed April 17, 1909.

approved form,

rIl he still does not emit sounds indicating' temperatures. It merely emits sounds l showing whether or'not water is present inside, the still'. It should also he noted that rammen aug. 2o, una.

serial No. 490,612. n

the production of low grades of rosin is due simply to the undue heating in the still, for the higher the still is heated the more colo phonic acid is formed which turns the rosin to a darker hue.

I have discovered certain critical points beyond which the temperature must not rise in order to prevent ca rbonization, and the operator by watching my temperature indieating means is therefore enabled to prevent the temperature rising beyond these critical points and therefore he is enabled to absolutely prevent any chai-ring or carbonization at all, and consequently, is enabled to produce first grades of rosin under all conditions. Further, it should be observed that l apply my process to all grades of the crude product regardless of its age. Under the old process differing variations were introduced according to the age of the product,

Vand also according to the ideas of the different operators. By my process, however, one invariable rule is given to the operators with the'certainty that eliicient results are sure to follow.

ln order that my process may be more fully understood, reference is had to the accompanying drawings forming a part` of this specification, and in which:

Figure l is a side view of a still and condenser attached thereto; Fig. 2 is a view, on a larger scale, showing the face plate of the thermometer; and, Fig. 3 is a cross sect-ion of a part of the still, showing the means for holding the thermometer.

a represents a still of any ordinary or to the top of which is connected one end of a condenser worm l), in a condenser C, alll being of the ordinary type. The lower part of t-he condenser c is provided with an inlet pipe (Z, through which water is supplied by any suitable means; e is an overflow pipe connected to the top of vthe condenser c and communicating with the gles, the horizontal part passing through the brick work and wall yof the still, as described and shown in my former Patent No. 900,575, dated Oct. G 1908. As shown in `Fig. Q, the face plate g is not only graduated as an ordinary Fahrenheit thermometer-lult also bears specific legends, all of iise in my -process. Thus besides the usual marks at every ten degrees, the point corresponding to the boiling point of Water is marked 212 and also Spirits indicating to the operator the point When the Water in the charge in the still (and incidentally the spirits of turpentine) begins to evaporate. Thus the 275 degree point is also marked and midway between this point and the' 250 degree point is the Word lllater7 With arrows leading vfrom this Word to the 250 and Q75 degree points, respectively. Then the 306 degree point is marked With the word Fluidity opposite it, and finally the 316 degree point is marked With the Word Limit opposite it. I prefer to use a mercury thermometer, but could use any form ot thermometer or pyrometer or indi',- cating device which will indicate with reasonable accuracy the temperatures inside the still. v

From a long series of experiments l have I discovered that when the crude gum is raised in the still to a temperature of about 2750 it. thatethe Water which is intimately and possibly chemically combined with the product, has been distilled oli', and that therefore, if the heating is continued Without water,carbonization or discoloration begins to take place. As this water is given off it is a matter of necessity that more water should be added, as otherwise the temperature will rapidly run up, resulting inevitably in carbonization. After the process is conducted steadily with the addition of small quantities of water for a considerable time, during 'which the teniperature is sloivly allowed toi-iss unt-il it reaches 25060 F., practically all ofthe spiiz'ts of turpentine and other volatile products, including the water, are driven ofi", great care being taken that the limit et 316C' F. should not-be exceeded. As a matter of fact, under the old process Whenever it was attempted to get out of the crude gum all. of the turpentine contained therein, the rosin was invaribly discolored and therefore its 'on'n'nercial'value larg ly destroyed. Acco rto my inveotiomluwever, these objections are all'obviatcd, an d in carrying out the same l in'efualily distil the crude gum up to say when Q F. isi-cached, and then begin to add .vater slowly, and especially after the point of QTL?" F. has been reached. The Water is added continuousljf and in small quantities after 275C F. has been reached and until 3060 F. is attained. The ten'ipcrature is thus prevented from ris-- ing too rapidly, and the gum is fort-,ed to give up all of its .spirits .vitho. any undue carbonization. rllhe time during which this water is added. will vary accordingto the Weight of the material being operated upon, but may roughly7 be stated in certain cases to extend over period of ahalf an hour to -an hour. After the temperature has reached 306 F. the distilling operation will have been practically completed as may be observe'd by the smallness of the quantity of spirits of turpentine which is being delivered from the Worm of the condenser. At the end of the process it is desirable to make the residue in the still perfectly fluid, and therefore ethe temperature is permitted to reach up to say 316 F. whereupon the same may be Withdrawn from the still and a new batch of :material introduced. Should the temperature be permitted to rise much beyond 3160 F. gas will be given ott', and the residue thus decomposed.

Theabove process was discovered after a series of experiments Which were satisfactorily continued for over a year, and which resulted in the disclosure of the fact that if the temperature is not allowed to rise above 260C F. only about yone-third of the spirits will distil over. These experiments further resulted in discovering the fact that unless water is added after a temperature of 2750 F. is reached all the turpentine and volatile products would not come off for the mass would settle down into a quiescent state Without any ebullition, and would remain in such a state until the heat rose above the danger point of 3160 F. after 1which gas wouldbe given od. From these experiments I have thus been enabled to formulate a definite system of rules for the distillation of crude gum, and to indicate the proper points on the face plate of a thermometer to show the operator what must be done to Carry out the process correctly.

Accordingtto my invention the temperature inside the still may at all times not only be accurately known by the operator, but may be regulated as Well. That is to say, the operator may at all times observe the thern'iometer, and thereby know with accarac),T the temperature ofthe contents of the still, vwhereupon when said temperature' rises or falls to an undesirable degree, he then regulates the cock f or other means, which controls the amount of Water admitted tothe still, and thereby brings the temperature back to the desired point, which usually in the neighborhood of 3060 F. t' course, in some instances, this regulation of temperature is aided by an increase or decrease in the amount of heaty admitted to the Those skilled in the art. Will be able to practise my invention from the above dis closure, but in order to make the process more clear, the following specific example is frivenz--uppose one 'has in the still l0 barrels or gallons of crude gum, and suppose the temperature has been observed to be about 260 inside the still, Water will new be added at the rate of about one gallon per minute and the time this water iis is permitted to dow into the still will deper minute.

pend upon the amount of gum being treated. lWith the barrelsabove supposed Water may be added for about an hour and Iii'teen minutes, during which time the temperature may be steadily increased at the rate ot about Six tenths (.6) of a degree n Ot course, the above eupposes that distillation has been going on for about minutes prior to the addition of Water, and during which L minutes the tempera# 'ture steadily increased from 212 to T600. li may cite as another Specific caseo barrel* of crude gum in the still, in which instance it would probably take 25 minutes to raise the temperature from 212 to 260O 'when W ater would be added at the rate of one gallon per minute for a period of about 35 to itl minutes during which time the temperature. will be steadily increased 'from '2600 to 3062r The process of distilling off turpentine from crude gum Which consists in subjecting said gum to a temperature'inside astill of substantially 260O E, then adding Water continuously7 and permitting the temperature to rise to a point not exceeding 306 F. whereupon the addition o Water is stopped, then allowing the temperature to rise to substantially 31Go F. inside'the still to soften the residue left in the still, and finally withdrawing Said residue from the Still, substantiall)T as described.

In testimony whereof, aliX my signature, in presence of two Witnesses.

. STEPHENS NEAL.

"Witnes-sesi y R. M. PARKER, L. B. JONES. 

